EP0776256B1 - Säurebehandlung von rostfreiem stahl - Google Patents

Säurebehandlung von rostfreiem stahl Download PDF

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Publication number
EP0776256B1
EP0776256B1 EP95935087A EP95935087A EP0776256B1 EP 0776256 B1 EP0776256 B1 EP 0776256B1 EP 95935087 A EP95935087 A EP 95935087A EP 95935087 A EP95935087 A EP 95935087A EP 0776256 B1 EP0776256 B1 EP 0776256B1
Authority
EP
European Patent Office
Prior art keywords
stainless steel
acid
water
iron ions
contact
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP95935087A
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English (en)
French (fr)
Other versions
EP0776256A1 (de
EP0776256A4 (de
Inventor
Sadiq Shah
Fred Kirchner
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Steris Inc
Original Assignee
Steris Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Steris Inc filed Critical Steris Inc
Publication of EP0776256A1 publication Critical patent/EP0776256A1/de
Publication of EP0776256A4 publication Critical patent/EP0776256A4/de
Application granted granted Critical
Publication of EP0776256B1 publication Critical patent/EP0776256B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/50—Treatment of iron or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C23G1/088—Iron or steel solutions containing organic acids

Definitions

  • the present invention relates to methods for cleaning and passivating stainless steel surfaces, such as gas flow equipment, pharmaceutical manufacturing equipment, and semiconductor processing equipment.
  • Chlorofluorocarbon cleaning solvents sold under the trademark Freon are examples of known cleaning solvents as well as 1,1,1-trichloroethane and methylene chloride.
  • Passivation of cleaned steel surfaces is important for preventing conditions such as flash rusting of cleaned wet steel.
  • cleaned steel is often passivated by treating with an nitric acid solution to provide altered surface characteristics that resist rusting.
  • Dilute solutions of citric acid made alkaline with ammonia or with an amine have been used for passivation of cleaned steel surfaces. These same solutions also have been used in combination with sodium nitrite.
  • Water-soluble amines are sometimes added to latex or water-dispersed coatings for steel to reduce corrosion. Water-soluble amines also have been added to final rinses for cleaned steel, but always in combination with other materials (such as other alkaline chemicals, citric acid, sodium nitrite, etc., and as exemplified in United States Patents 3,072,502; 3,154,438; 3,368,913; 3,519,458; and 4,045,253) and therefore these rinses have left insoluble residues on the steel surfaces that are detrimental to optimum performance of subsequently applied protective coatings.
  • other materials such as other alkaline chemicals, citric acid, sodium nitrite, etc.
  • cleaned steel is often passivated by treating with an alkaline sodium nitrite solution to provide altered surface characteristics that resist rusting.
  • United States Patent 4,590,100 describes a process that allows previously cleaned steel to be passivated with a rinse of almost pure water, that is made slightly alkaline with an amine to inhibit corrosion preparatory to application of non-aqueous protective coatings, such that any small amine residue remaining on the steel surface after drying of the water will itself evaporate and in such a manner that any remaining amine residue will be incorporated into the non-aqueous protective coating without leaving any water-soluble or ionic residue on the surface of the steel.
  • United States Patents 5,252,363 and 5,321,061 describe aqueous organic resin-containing compositions which are useful for depositing coatings on freshly galvanized metals to protect the metals against white rust and provide a surface which is universally paintable.
  • the organic resin consists essentially of at least one water-dispersible or emusifiable epoxy resin or a mixture of resins containing at least one water-dispersible or emulsifiable epoxy resin.
  • United States Patent 5,039,349 describes a method and apparatus for cleaning surfaces, such as semiconductor processing equipment and pharmaceutical processing equipment, to absolute or near-absolute cleanliness involving spraying jets of heated cleaning solution so that it flows over and scrubs the surfaces to be cleaned, producing a rinse liquid.
  • the rinse liquid is filtered and recirculated over the surface to be cleaned.
  • the invention is a method for treating stainless steel that both cleans and passivates the stainless steel surface.
  • the present invention teaches a method for concurrently cleaning a residue from and passivating a stainless steel surface which includes iron ions, the method comprising:
  • the surfactant is selected from the group consisting of anionic, cationic, non-ionic and zwitterionic surfactants to enhance cleaning performance.
  • the method for treating stainless steel according to the present invention includes contacting a composition comprising an acid component and water to the stainless steel surface.
  • the compositions treat the stainless steel surface by removing residue, formed on the stainless steel surface during use of the stainless steel surface (e.g., during pharmaceutical or semiconductor processing), from the surface, simultaneously complexing free iron ions liberated from the stainless steel steel surface and forming an oxide film on the stainless steel surface, and precipitating the complexed ions into the oxide film.
  • compositions useful for the methods of the invention consist of 1 and 60% acid component, 1-15% surfactant, and between 39 and 98% water. Unless otherwise indicated, all amounts are percentages are weight/weight.
  • the surfactant is selected from the group consisting of anionic, cationic, nonionic and zwitterionic surfactants to enhance cleaning performance.
  • surfactants include but are not limited to water-soluble salts or higher fatty acid monoglyceride monosulfates, such as the sodium salt of the monosulfated monoglyceride of hydrogenated coconut oil fatty acids, higher alkyl sulfates such as sodium lauryl sulfate, alkyl aryl sulfonates such as sodium dodecyl benzene sulfonate, higher alkyl sulfoacetates, higher fatty acid esters of 1,2 dihydroxy propane sulfonates, and the substantially saturated higher aliphatic acyl amides of lower aliphatic amino carboxylic acid compounds, such as those having 12 to 16 carbons in the fatty acid, alkyl or acyl radicals, and the like.
  • amides are N-lauroyl sarcosine, and the sodium, potassium, and ethanolamine salts of N-lauroyl, N-myristoyl, or N-palinitoyl sarcosine.
  • condensation products of ethylene oxide with various reactive hydrogen-containing compounds reactive therewith having long hydrophobic chains e.g. aliphatic chains of about 12 to 20 carbon atoms
  • condensation products e.g. aliphatic chains of about 12 to 20 carbon atoms
  • ethoxamers contain hydrophilic polyoxyethylene moieties, such as condensation products of poly (ethylene oxide) with fatty acids, fatty alcohols, fatty amides, polyhydric alcohols (e.g. sorbitan monostearate) and polypropyleneoxide (e.g. Pluronic materials).
  • Miranol JEM an amphocarboxylate surfactant available from Rhone-Poulenc, Cranbury, New Jersey, is a typically suitable surfactant.
  • Acid components suitable for the present invention are hydroxyacetic acid and citric acid.
  • Acetic acid is not suitable for the method of the invention.
  • the compositions can include more than one acid component.
  • Water suitable for the present invention can be distilled water, soft water, or hard water.
  • Methods of the present invention for cleaning and passivating a stainless steel surface comprise:
  • both cleansing and passivation are achieved within about 20-30 minutes of initial treatment.
  • the method comprises:
  • the method comprises:
  • the method comprises
  • materials such as pharmaceutical products present in stainless steel manufacturing vessels to be cleaned and passivated are removed from the vessel. While the bulk of the material to be removed readily flows from the stainless steel vessel, a residue film remains on the stainless steel surface.
  • compositions used in the present invention are contacted with the film-coated surface in one or more of several ways.
  • One way to contact the film-coated surface is by using a fixed spray-ball mechanism which showers the composition onto the film-coated surface such that all film-coated surfaces are contacted with the composition.
  • Another way to contact the film-coated surface is by using a flexible spray-ball mechanism which, at various positions within the vessel, showers the composition onto the film-coated surface such that all film-coated surfaces are contacted with the composition.
  • Another way is to fill the vessel such that all film-coated surfaces are contacted with the composition.
  • the film is dislodged and solubilized, dispersed, or emulsified into the composition and removed from the vessel. Free iron ions are liberated from the surface and form an oxide film on the surface The complexed ions of iron are precipitated into the oxide film.
  • the composition removed from the vessel is optionally discarded or recycled.
  • stainless steel can be cleaned and passivated in one treatment.
  • the method provides a passive protective film in addition to cleaning stainless steel surfaces.
  • Table 2 in Example 2 represents data obtained from studies evaluating the passivation properties obtained using methods of the invention.
  • Corrosion rate measured electrochemically in mils per year (MPY)
  • MPY mils per year
  • Subsequent exposure of these passivated electrodes to fresh solutions of the same formulation results in no rise in corrosion rate, due to the protective effect of the passive film previously formed.
  • As the corrosion reaction is initiated the free iron ions liberated are complexed.
  • An oxide film forms on the metal surface upon exposure to the acid component. The complexes readily precipitate and incorporate into the oxide film, enhancing the integrity of the oxide film.
  • Stainless steel 316 electrodes were treated with a 34% nitric acid solution, a standard solution used for passivating stainless steel surfaces.
  • a corrosion rate profile was generated by immersing the electrodes in a fresh diluted solution and monitoring the corrosion rate, as measured in mils per year. The profile showed initial corrosion for a short period of time, resulting in formation of a protective film, followed by an extended period of time showing virtually no additional corrosion.
  • compositions having the following formulations were prepared by adding acid to water: Formulation 1 2 3
  • Ingredient Acetic acid 23.2% - - Hydroxyacetic acid - 29.4% - Citric acid - - 25.5%
  • Miranol JEM 2.0 2.0 2.0 Water 74.8 68.6 72.5 Total 100% 100%
  • Each formulation was evaluated by diluting to a concentration of 31 ml/liter, immersing stainless steel 316 electrodes to the diluted formulation at 80°C, and continuing to monitor the corrosion rate. Water alone was also evaluated. Table 2 shows the corrosion rate achieved using Formulations 1, 2, or 3 described in Table 1, or water.
  • Corrosion rate ⁇ m/year (mils/year) 1 2 3 water Time 1 minute 0 (0.0) 102 (4.0) 25 (1.0) 1 (0.05) 2 minutes 51 (2-0) 203 (8.0) 102 (4.0) 1 (0.05) 3 minutes 51 (2.0) 51 (2.0) 203 (8.0) 1 (0.05) 4 minutes 51 (2.0) 25 (1.0) 51 (2.0) 1 (0.05) 5 minutes 51 (2.0) 25 (1.0) 25 (1.0) 1 (0.05) 10 minutes 18 (0.7) 18 (0.7) 18 (0.7) 1 (0.05) 15 minutes 10 (0.5) 10 (0.5) 10 (0.5) 1 (0.05) 30 minutes 10 (0-5) 10 (0.5) 10 (6-5) 1 (0.05) 60 minutes 8 (0.3) 8 (0.3) 8 (0.3) 1 (0.05)

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Detergent Compositions (AREA)

Claims (4)

  1. Ein Verfahren zum gleichzeitigen Entfernen eines Rückstands von und Passivieren einer Edelstahloberfläche, die Eisenionen umfasst, wobei das Verfahren umfasst:
    (1) In-Kontakt-Bringen der Edelstahloberfläche mit 15 bis 45 ml pro Liter einer Säureformulierung, wobei die Säureformulierung aus zwischen 1 und 60 % (Gew./Gew.) aus mindestens einer von einer Hydroxyessigsäure- oder Zitronensäurekomponente, zwischen 1 und 15 % (Gew./Gew.) eines oberflächenaktiven Mittels und zwischen 39 und 98 % (Gew./Gew.) Wasser besteht,
    (2) Aufrechterhalten des Kontakts zum Lösen und Entfernen des Rückstands und zum Freisetzen freier Eisenionen von der Edelstahloberfläche, und
    (3) Fortsetzen des Kontakts zur Bildung eines passiven Schutzfilms auf der Oberfläche, der einen Teil der Eisenionen in Oxidform und einen Teil der Eisenionen, die durch die Säurekomponente komplexiert sind, umfasst,
    wodurch eine Oberfläche ohne Rückstand, die bezüglich einer weiteren Oxidation im Wesentlichen passiv ist, bereitgestellt wird.
  2. Verfahren nach Anspruch 1, bei dem die Oberfläche mit 22 bis 38 ml pro Liter der Säureformulierung in Kontakt gebracht wird, wobei die Säureformulierung zwischen 15 und 40 % (Gew./Gew.) der Komponente, zwischen 1 und 15 % (Gew./Gew.) des oberflächenaktiven Mittels und zwischen 59 und 84 % (Gew./Gew.) Wasser umfasst.
  3. Verfahren nach Anspruch 1 oder 2, bei dem die Säurekomponente Hydroxyessigsäure ist.
  4. Verfahren nach Anspruch 1, bei dem die Edelstahloberfläche innerhalb von 20 bis 30 min gereinigt und passiviert wird.
EP95935087A 1994-09-26 1995-09-22 Säurebehandlung von rostfreiem stahl Expired - Lifetime EP0776256B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US31180894A 1994-09-26 1994-09-26
US311808 1994-09-26
PCT/US1995/012182 WO1996009899A1 (en) 1994-09-26 1995-09-22 Stainless steel acid treatment

Publications (3)

Publication Number Publication Date
EP0776256A1 EP0776256A1 (de) 1997-06-04
EP0776256A4 EP0776256A4 (de) 1998-05-20
EP0776256B1 true EP0776256B1 (de) 2005-07-27

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP95935087A Expired - Lifetime EP0776256B1 (de) 1994-09-26 1995-09-22 Säurebehandlung von rostfreiem stahl

Country Status (9)

Country Link
US (1) US5766684A (de)
EP (1) EP0776256B1 (de)
JP (1) JP2941948B2 (de)
AT (1) ATE300630T1 (de)
AU (1) AU3724095A (de)
CA (1) CA2200587C (de)
DE (1) DE69534340T2 (de)
ES (1) ES2247593T3 (de)
WO (1) WO1996009899A1 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007010538A1 (de) * 2007-03-05 2008-09-11 Poligrat Gmbh Verfahren zum thermochemischen Passivieren von Edelstahl
DE102012107807A1 (de) * 2012-08-24 2014-02-27 Paul Hettich Gmbh & Co. Kg Verfahren zur Herstellung eines metallischen Bauteils eines Beschlages, Ofenbeschlag und Ofen mit Pyrolysereinigungsfunktion

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US6770150B1 (en) 2000-03-09 2004-08-03 Steris Inc. Process for removing deposits from enclosed chambers
US6341612B1 (en) 2000-03-09 2002-01-29 Steris Inc Two compartment container for neutralizing used cleaning solutions
US6550487B1 (en) 2000-03-09 2003-04-22 Steris Inc. Apparatus for removing deposits from enclosed chambers
US6506254B1 (en) 2000-06-30 2003-01-14 Lam Research Corporation Semiconductor processing equipment having improved particle performance
US6890861B1 (en) 2000-06-30 2005-05-10 Lam Research Corporation Semiconductor processing equipment having improved particle performance
US20050234545A1 (en) * 2004-04-19 2005-10-20 Yea-Yang Su Amorphous oxide surface film for metallic implantable devices and method for production thereof
ES2286938B1 (es) * 2006-04-26 2008-11-01 Supramol.Lecular Systems S.L. Solucion electrolitica para el pulido electroquimico de articulos de metal.
KR100744639B1 (ko) * 2006-07-31 2007-08-07 주식회사 월덱스 실리콘 단일재질의 플라즈마 챔버 캐소드 및 아웃링
EP2182095A1 (de) 2008-10-29 2010-05-05 Poligrat Gmbh Verfahren zur Oberflächenbehandlung von nichtrostendem Stahl
DK2576868T3 (en) * 2010-05-27 2018-10-29 Mj Liquid Solutions Inc PROCEDURE FOR TREATING ARTICLES OF ROLLED STEEL
US8734586B2 (en) 2012-02-02 2014-05-27 Sematech, Inc. Process for cleaning shield surfaces in deposition systems
US8734907B2 (en) 2012-02-02 2014-05-27 Sematech, Inc. Coating of shield surfaces in deposition systems
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Publication number Priority date Publication date Assignee Title
DE102007010538A1 (de) * 2007-03-05 2008-09-11 Poligrat Gmbh Verfahren zum thermochemischen Passivieren von Edelstahl
US8430973B2 (en) 2007-03-05 2013-04-30 Poligrat Gmbh Method for the thermochemical passivation of stainless steel
DE102012107807A1 (de) * 2012-08-24 2014-02-27 Paul Hettich Gmbh & Co. Kg Verfahren zur Herstellung eines metallischen Bauteils eines Beschlages, Ofenbeschlag und Ofen mit Pyrolysereinigungsfunktion

Also Published As

Publication number Publication date
WO1996009899A1 (en) 1996-04-04
JP2941948B2 (ja) 1999-08-30
DE69534340T2 (de) 2006-04-20
AU3724095A (en) 1996-04-19
CA2200587C (en) 2001-02-27
EP0776256A1 (de) 1997-06-04
ES2247593T3 (es) 2006-03-01
US5766684A (en) 1998-06-16
EP0776256A4 (de) 1998-05-20
JPH10503240A (ja) 1998-03-24
CA2200587A1 (en) 1996-04-04
ATE300630T1 (de) 2005-08-15
DE69534340D1 (de) 2005-09-01

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